杨木屑硫酸水解的研究

对杨木屑分别进行浓硫酸和稀硫酸水解,稀硫酸水解时水解温度为200℃,硫酸质量分数为2.5%时,得糖率最高为64.5%;浓硫酸水解时水解温度为60℃,硫酸质量分数为70%,得糖率可达到96.4%。采用低酸固比硫酸水解杨木屑,考察水解温度、时间及二次水解时间对得糖率的影响,结果表明:较好的条件是水解温度95℃,时间0.5h,二次水解时间2h,得糖率可达到61.9%。此方法与浓硫酸、稀硫酸水解相比较,耗酸量少,反应条件较温和,能取得较好的水解效果。     

从植物水解冷凝液分离糠醛和乙酸——两步萃取流程的开发

<正> 从含有多缩戊糖的植物废料水解制取糠醛的工业生产,已有近70年的历史。目前全世界糠醛年产量已达25万吨。但是植物水解冷凝液的浓度很低,一般含糠醛4～6％,乙酸1～2％,还有少量低沸物。国内外均用蒸馏法提纯,其中的醋酸经中和后排走,关于萃取法的研究,总共发表了37种溶剂对糠醛水溶液的平衡分配系数,现将其归纳如下: 奥地利在82～86年间,提出了三步法萃取流程。即:①用氯仿萃取糠醛②用煤油将萃余水相中溶解的氯仿(0.6％wt)萃取出来③用以叔胺为基础的三元混合溶剂萃取水     

在乙酸丁酯-水双相体系中玉米芯水解制备糠醛

以玉米芯为原料、硫酸铁为催化剂、乙酸丁酯为萃取剂,在乙酸丁酯-水双相体系中水解制备糠醛。考察了反应时间、催化剂浓度(硫酸铁溶液质量分数)、反应温度以及萃取剂与溶剂体积比对糠醛产率的影响,确定最佳工艺条件为:反应时间3.0h,催化剂浓度10%,反应温度160℃,萃取剂与溶剂体积比为4,在此条件下,糠醛产率达到43.49%。     

竹黄两种预水解制备糠醛的工艺比较研究

为使竹屑资源得到充分利用,对两种预水解制备糠醛的工艺进行了比较探究。首先采用亚硫酸氢钠预处理和稀酸预处理对半纤维素进行提取,然后研究了反应温度、反应时间、硫酸浓度、戊糖初始浓度和NaCl用量对糠醛收率的影响,最后对水解底物的酶解效果进行了初步探究。在相同的酶解条件下,亚硫酸氢钠预水解底物酶解率高于稀酸水解底物酶解率。     

亚/超临界乙醇条件下杨木屑与甘油共液化研究

以60～80目的杨木屑为原料,甘油为液化剂,酸为催化剂,基于超临界乙醇条件下对杨木屑进行液化制备生物重油。实验结果表明:以2.5%硫酸为催化剂,在甘油/乙醇/木屑质量比为5∶10∶2条件下,250℃反应1 h,木屑的转化率可达98%。此液化油含水量为3.04%(wt),运动黏度为524 mm2/s,酸值为2.1 mg KOH/g,羟值为846 mg KOH/g。对液化油进行IR、GPC和GC-MS分析的结果显示,液化油含有大量的羟基物质,平均相对分子质量为811,并且含有4-羰基戊酸丁酯、三乙基甘油醚等聚酯/聚醚类多元醇。     

树脂催化水解制备固体氰乙酸的工艺研究

介绍了一种合成固体氰乙酸的新工艺。该工艺以氰乙酸乙酯为原料,经732型阳离子交换树脂催化,通过水解制备固体氰乙酸。考察了反应温度,反应时间,氰乙酸乙酯和水的质量比和氰乙酸乙酯和树脂的质量比对反应的影响。结果表明,最佳的反应条件为:反应温度为90℃,反应时间为10h,水酯质量比为1∶1,酯与树脂质量比为10∶4.5,在该条件下,氰乙酸的最高收率可达88.9%。     

磷酸活化法制备糠醛渣活性炭的研究

以碘吸附值、亚甲基蓝吸附值及活性炭得率为考察指标,选取对糠醛渣活性炭性质影响较大的浸渍比、磷酸质量分数、活化温度、保温时间4个因素进行L₁₆(4⁵)正交试验对磷酸活化法制备糠醛渣活性炭的工艺条件进行优化。由正交试验结果得到磷酸活化的最佳工艺条件为:磷酸质量分数60%,浸渍比2.5:1,活化温度550 ℃,保温1.5 h,此条件下制得的活性炭样品的碘吸附值为839.6 mg/g,亚甲基蓝吸附值为260.3 mg/g,得率为46.8%,比表面积为830.20 m²/g,孔容积为0.502 cm³/g,孔径集中在0.8~2.5 nm,具有丰富的中孔和微孔。     

搅拌水解对糠醛收率的影响

通过两种生产工艺的对比实验,证明采用搅拌水解新工艺,可以强化水解过程,减少糠醛在高温下产生分解反应;可以更新物料表面层,减少醛汽同酸性介质的接触,减少糠醛的树脂化,从而提高玉米芯水解制取糠醛的收率     

花生壳常压水解制糠醛工艺研究

本文研究了花生壳制糠醛的可行性。在常压下,用液／固比为5：1、5％N35％的H2SO4水溶液水解花生壳,考察了催化剂（TiO2、ZnCl2和FeCl3）、反应时间和蒸馏方式对糠醛产率的影响。实验结果表明,FeCl3催化效果最好,TiO2最差,H2SO4的最佳浓度为25％。在此条件下,加入3％的FeCl3,恒定体积（连续补水）蒸馏90min,然后在50min内蒸干,糠醛收率可达7．0％,大约为理论收率的70％。     

玉米芯水解制备糠醛的研究

对玉米芯水解制备糠醛进行了研究。采用硫酸铁作催化剂,通过单因素实验研究了添加剂种类及用量、反应时间、反应温度对糠醛得率的影响。确定制备糠醛的最佳工艺条件为:催化剂硫酸铁浓度10%(质量分数),选用KI为添加剂,添加量0.3mol·L-1,反应温度180℃,反应时间150min,在此条件下糠醛得率可达52.54%。     

Sugarcane bagasse hydrolysis with phosphoric and sulfuric acids and hydrolysate detoxification for xylitol production

The effectiveness of phosphoric acid to release xylose from sugarcane bagasse hemicellulose was assessed through a 2³ full factorial design. The maximum xylose concentration in the hydrolysate (17.1 g dm^?3) was attained when the bagasse was treated at 160 °C for 60 min, using 70 mg of phosphoric acid per gram of dry‐bagasse. Hydrolysis carried out with sulfuric acid, under optimum conditions previously determined, provided a hydrolysate with a similar xylose concentration (17.2 g dm^?3). After vacuum concentration, these hydrolysates were detoxified and used for xylitol production with the yeast Candida guilliermondii. Two different detoxification strategies, which consisted of adjusting the pH of the hydrolysates to 5.5 with either calcium oxide or ammonium hydroxide, both followed by active charcoal adsorption, were tested. The best xylitol productions (18.1 and 19.2 g dm^?3) were observed when calcium oxide was used to adjust the pH of both the phosphoric and the sulfuric acid hydrolysates, respectively. Copyright © 2004 Society of Chemical Industry     

甲酸/乙酸/氯化钠催化玉米芯水解条件优化

为解决目前糠醛行业使用无机酸做催化剂存在的严重污染及收率低等问题,提出两步法有机酸/无机盐复合体系催化玉米芯水解生产糠醛新工艺。文中以获得第1步水解玉米芯过程中较高的五碳糖收率和低的糠醛质量浓度为目的。研究了反应温度、反应时间、酸质量分数及氯化钠浓度对玉米芯中半纤维素水解的影响。通过响应曲面法,对水解条件进行了优化,建立了糖收率和糠醛质量浓度的2个二次多项式模型。由响应面分析和模型方程优化得出玉米芯水解的最佳水解条件:反应时间90 min、氯化钠浓度1.5 mol/L、温度134.7℃和酸质量分数为4.67%,此时糖收率为36%、糠醛质量浓度为1.98 g/L,为下一步五碳糖水解生产糠醛提供了较为满意的糖质量浓度和糠醛质量浓度,同时在最佳水解条件下的验证实验结果与模型预测值十分接近,说明模型是适用的。     

Further aspects of powdered poplar wood liquefaction by aqueous pyrolysis

The liquefaction of powdered poplar wood by rapid pyrolysis in water at 350°C has been studied further. It differs significantly from the liquefaction of wood chips in that oil yields are improved by pressurisation of the reactor. Oil yields (chloroform soluble) are about 45 per cent and are sensitive to water/wood mass ratios and residence time. Gas, measured in a new handling system, is produced in 5–12 per cent mass yields and contains 86–90 per cent carbon dioxide and 10–13 per cent carbon monoxide. The oil and aqueous phases contain carboxylic acids (particularly acetic), phenols, cyclohexanones, cyclopentanones, benzyl alcohols and furfural.     

醋酸水解玉米芯中木聚糖的动力学

利用醋酸作为催化剂水解玉米芯中半纤维素来制备还原糖,测定了温度在160-200℃、固液质量比为1∶15、搅拌速度为500 r/min下,不同水解时间水解液中还原糖的收率以及副产物糠醛的收率.利用半纤维素高温液态水的Garrote模型拟合还原糖生成过程.实验表明,该模型能够较好地描述还原糖生成过程以及副产物糠醛的产生过程...     

管式环流反应器在乙酸/乙酐羰基合成中的应用

介绍了以乙酸甲酯和甲醇为原料合成年产20 kt乙酐和20 kt乙酸的过程,并且介绍了在以LiI为促进剂的铑-碘均相催化剂作用下、170~199℃的温度范围及5.0 MPa压力条件下,管式环流反应器在乙酸/乙酐合成中的应用。分析了反应器内流体的流动特点和羰基合成的反应过程,建立了数学模型。计算得到了反应器内反应物料转化率、各组分浓度、温度和冷却水温度等各种参数沿物料流动方向的分布,同时对反应器进行了热稳定性分析。计算结果表明,当系统在操作过程中转化率偏离定常态0.000 1,温度偏离定常态0.000 1℃时,转化率和温度能分别在4×10-6s和8×10-6s内回到定常态,整个反应体系是稳定的。     

An effective rhodium catalyst system on the synthesis of acetic acid from methyl formate

Rh/Lil/SnR₄ is an effective catalyst system for the conversion of methyl formate to acetic acid under carbon monoxide pressure. The effects of solvent and initial CO partial pressure on the turnover rate of the reaction were investigated. The possibility of replacing some of the iodide promoters by tin compounds has been probed.     

Electrochemical synthesis of poly(ortho-ethoxyaniline) from phosphoric and sulphuric acid solutions

The growth and nucleation mechanism of poly(ortho-ethoxyaniline) (POEA) are investigated by cyclic voltammetry (CV) and potentiostatic technique. It was shown that growing of POEA is faster in sulphuric acid solution compared to phosphoric acid solution. Different rate trends were obtained with the increase of switching potential. From cyclic voltammograms, it is evident that the obtained polymer has a similar behaviour to the one reported for polyaniline, but there is a difference in position of current peaks, due to the electronic and steric effects of ethoxy-group. In presence of different anions, a different nucleation mechanism was obtained. In sulphuric acid solution nucleation proceeds through 3D instantaneous nucleation under diffusion control, and in phosphoric acid solution nucleation proceeds through 3D progressive nucleation under diffusion control.     

近临界水中水解鱼蛋白制备氨基酸

The hydrolysis technology and reaction kinetics for amino acids production from fish proteins in subcritical water reactor without catalysts were investigated in a reactor with volume of 400 ml under the conditions of reaction temperature from 180-320℃, pressure from 5-26 MPa, and time from 5-60 rain. The quality and quantity of amino acids in hydrolysate were determined by bioLiquid chromatography, and 17 kinds of amino acids were obtained. For the important 8 amino acids, the experiments were conducted to examine the effects of reaction temperature, pressure and time on amino acids yield. The optimum conditions for high yield are obtained from the experimental results. It is found that the nitrogen and carbon dioxide atmosphere should be used for leucine, isoleucine and histidine production while the air atmosphere might be used for other amino acids. The reaction time of 30 rain and the experimental temperature of 220℃, 240℃ and 260℃ were adopted for reaction kinetic research. The total yield of amino acids versus reaction time have been examined experimentally. According to these experimental data and under the condition of water excess, the macroscopic reaction kinetic equation of fish proteins hydrolysis was obtained with the hydrolysis reaction order of 1.615 and the rate constants being 0.0017, 0.0045 and 0.0097 at 220℃, 240℃ and 260℃ respectively. The activation energy is 145.1 kJ·mol^- 1.